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JP2004358466A5
JP2004358466A5 JP2004168839A JP2004168839A JP2004358466A5 JP 2004358466 A5 JP2004358466 A5 JP 2004358466A5 JP 2004168839 A JP2004168839 A JP 2004168839A JP 2004168839 A JP2004168839 A JP 2004168839A JP 2004358466 A5 JP2004358466 A5 JP 2004358466A5
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stream
solvent
mother liquor
zone
water
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JP2004358466A (en
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Priority claimed from US10/455,016 external-priority patent/US7410632B2/en
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固液分離工程は、超濃縮母液流１４５を固液分離ゾーン１５１に供給して、有機不純物１４６、水性流１４７及び第２水性流１４８を生成せしめることを含む。固液分離ゾーン１５１は、少なくとも１つの固液分離装置を含む。使用する固液分離装置の形式には制限はない。このような装置の例としては、濾過装置及び遠心分離機が挙げられるが、これらに限定するものではない。水性流１４７は、超濃縮母液流１４５の濾過によって生成する。 The solid-liquid separation step comprises supplying super-concentrated mother liquor stream 145 to solid-liquid separation zone 151 to produce organic impurities 146, aqueous stream 147 and second aqueous stream 148. The solid-liquid separation zone 151 includes at least one solid-liquid separation device. There is no limitation on the type of solid-liquid separation device used. Examples of such devices include, but are not limited to , filtration devices and centrifuges . Aqueous stream 147 is produced by filtration of super-concentrated mother liquor stream 145.

Claims (25)

（ａ）第１蒸発器ゾーンにおいて、カルボン酸、金属触媒、不純物、水及び溶媒を含む母液を蒸発させて、蒸気流と濃縮母液流を生成せしめ；
（ｂ）第２蒸発器ゾーンにおいて、前記濃縮母液流を蒸発させて、溶媒高含有流及び超濃縮母液流を形成せしめ；
（ｃ）固液分離ゾーンにおいて、水溶媒溶液によって前記超濃縮母液から有機不純物を分離して、水性流と第２水性流とを形成せしめ；
（ｄ）混合ゾーンにおいて、水及び、場合によっては抽出溶媒、と前記水性流及び前記第２水性流とを混合して、水性混合物を形成せしめ；
（ｅ）抽出ゾーンにおいて、前記水性混合物に抽出溶媒を添加して、抽出物流及びラフィネート流を形成せしめ；そして
（ｆ）分離ゾーン中で前記抽出物流を分離して、高沸点有機不純物流及び回収抽出溶媒流を形成せしめる
各工程を含んでなる母液から金属触媒を回収する方法。 (A) Evaporating the mother liquor containing carboxylic acid, metal catalyst, impurities, water and solvent in the first evaporator zone to produce a vapor stream and a concentrated mother liquor stream;
(B) evaporating the concentrated mother liquor stream in the second evaporator zone to form a solvent rich stream and a superconcentrated mother liquor stream;
(C) separating the organic impurities from the superconcentrated mother liquor by an aqueous solvent solution in a solid-liquid separation zone to form an aqueous stream and a second aqueous stream;
(D) mixing the water and optionally the extraction solvent, and the aqueous stream and the second aqueous stream in the mixing zone to form an aqueous mixture;
(E) adding an extraction solvent to the aqueous mixture in the extraction zone to form an extract stream and a raffinate stream; and (f) separating the extract stream in a separation zone to obtain a high boiling point organic impurity stream and recovery A method of recovering a metal catalyst from a mother liquor comprising the steps of forming an extraction solvent stream . 前記工程（ａ）において、前記母液から前記溶媒及び水の５０〜８０重量％を除去する請求項１に記載の方法。   The method according to claim 1, wherein 50 to 80 wt% of the solvent and water are removed from the mother liquor in the step (a). 前記工程（ａ）及び（ｂ）において、合わせて、前記母液から前記溶媒及び水の７５〜９９重量％を除去する請求項２に記載の方法。   The method according to claim 2, wherein in the steps (a) and (b), 75 to 99% by weight of the solvent and water are removed from the mother liquor in combination. 前記工程（ａ）及び（ｂ）において、合わせて、前記母液から前記溶媒及び水の８５〜９９重量％を除去する請求項１に記載の方法。   The method according to claim 1, wherein in the steps (a) and (b), together, 85 to 99% by weight of the solvent and water are removed from the mother liquor. 前記工程（ａ）及び（ｂ）において、合わせて、前記母液から前記溶媒及び水の９０〜９９重量％を除去する請求項１に記載の方法。   The method according to claim 1, wherein in the steps (a) and (b), together, 90 to 99% by weight of the solvent and water are removed from the mother liquor. ２０〜７０℃の温度範囲において、前記水−溶媒溶液を固液分離ゾーンに添加する請求項１に記載の方法。   The method according to claim 1, wherein the water-solvent solution is added to the solid-liquid separation zone in a temperature range of 20-70 ° C. ３０〜５０℃の温度範囲において、前記水−溶媒溶液を固液分離ゾーンに添加する請求項１に記載の方法。   The method according to claim 1, wherein the water-solvent solution is added to the solid-liquid separation zone in a temperature range of 30 to 50 ° C. 前記抽出ゾーンが向流抽出装置を含む請求項1に記載の方法。   The method according to claim 1, wherein the extraction zone comprises a countercurrent extraction device. 前記抽出ゾーンが一段抽出装置を含む請求項1に記載の方法。   The method according to claim 1, wherein the extraction zone comprises a single stage extractor. 前記溶媒高含有流が酢酸ｎ−プロピル、酢酸イソプロピル、酢酸イソブチル、酢酸ｓｅｃ−ブチル、酢酸エチル及び酢酸ｎ−ブチルからなる群から選ばれる溶媒を含む請求項１に記載の方法。   The method according to claim 1, wherein the high solvent content stream comprises a solvent selected from the group consisting of n-propyl acetate, isopropyl acetate, isobutyl acetate, sec-butyl acetate, ethyl acetate and n-butyl acetate. 前記第２蒸発器ゾーンが２０〜７０℃の温度で運転される蒸発器を含む請求項１に記載の方法。   The method according to claim 1, wherein the second evaporator zone comprises an evaporator operated at a temperature of 20-70C. 前記蒸発器が真空条件において運転される請求項９に記載の方法。   10. The method of claim 9, wherein the evaporator is operated at vacuum conditions. 請求項１に記載の方法によって製造される超濃縮母液流。   A superconcentrated mother liquor stream produced by the method of claim 1. 請求項１に記載の方法によって製造される水性混合物。   An aqueous mixture produced by the method of claim 1. 請求項１に記載の方法によって製造されるラフィネート流。   A raffinate stream produced by the method of claim 1. 請求項１に記載の方法によって製造される抽出物流。   An extract stream produced by the method of claim 1. 請求項１に記載の方法によって製造される回収抽出溶媒流。   A recovered extraction solvent stream produced by the method of claim 1. 請求項１に記載の方法によって製造される高沸点有機不純物流。   A high boiling organic impurity stream produced by the method of claim 1. （ａ）第１蒸発器ゾーンにおいて、カルボン酸、金属触媒、不純物、水及び溶媒を含む母液を蒸発させて、蒸気流と濃縮母液流を生成せしめ；そして
（ｂ）第２蒸発器ゾーンにおいて、前記濃縮母液流を蒸発させて、溶媒高含有流及び超濃縮母液流を生成せしめる（工程（ａ）と工程（ｂ）の蒸発によって合わせて溶媒の９５〜９９重量％が母液から除去され；第２蒸発ゾーンは２０〜７０℃の温度で運転される蒸発器を含む）
各工程を含んでなる超濃縮母液流の製造方法。 (A) evaporating the mother liquor containing carboxylic acid, metal catalyst, impurities, water and solvent in the first evaporator zone to produce a vapor stream and a concentrated mother liquor stream; and (b) in the second evaporator zone The concentrated mother liquor stream is evaporated to produce a solvent rich stream and a superconcentrated mother liquor stream (combined by the evaporation of step (a) and step (b) 95 to 99% by weight of the solvent is removed from the mother liquor; 2Evaporation zone includes an evaporator operated at a temperature of 20-70 ° C)
A method of producing a superconcentrated mother liquor stream comprising each step. 前記第２蒸発器ゾーンが真空条件において運転される蒸発器を含む請求項１９に記載の方法。   20. The method of claim 19, wherein the second evaporator zone comprises an evaporator operated at vacuum conditions. （ａ）第１蒸発器ゾーンにおいて、カルボン酸、金属触媒、不純物、水及び溶媒を含む母液を蒸発させて、蒸気流と濃縮母液流を生成せしめ；
（ｂ）第２蒸発器ゾーンにおいて、前記濃縮母液流を蒸発させて、溶媒高含有流及び超濃縮母液流を形成せしめ（工程（ａ）と工程（ｂ）において合わせて溶媒の８５〜９９重量％が母液から除去される）；
（ｃ）固液分離ゾーンにおいて、水−溶媒溶液によって前記超濃縮母液から有機不純物を分離して、水性流と第２水性流を形成せしめ（前記水−溶媒溶液は２０〜７０℃の温度範囲において固液分離ゾーンに添加される）；
（ｄ）混合ゾーンにおいて、水及び、場合によっては抽出溶媒、と前記水性流及び前記第２水性流とを混合して、水性混合物を形成せしめ；
（ｅ）抽出ゾーンにおいて、前記水性混合物に抽出溶媒を添加して、抽出物流及びラフィネート流を形成せしめ；そして
（ｆ）分離ゾーンにおいて抽出物流を分離して、高沸点有機不純物流及び回収抽出溶媒流を形成せしめる
各工程を含んでなる母液から触媒を回収する方法。 (A) Evaporating the mother liquor containing carboxylic acid, metal catalyst, impurities, water and solvent in the first evaporator zone to produce a vapor stream and a concentrated mother liquor stream;
(B) in the second evaporator zone, evaporating the concentrated mother liquor stream to form a solvent rich stream and a superconcentrated mother liquor stream (85-99 weight of solvent combined in steps (a) and (b) % Is removed from the mother liquor);
(C) In the solid-liquid separation zone, organic impurities are separated from the super-concentrated mother liquor by a water-solvent solution to form an aqueous stream and a second aqueous stream (the water-solvent solution has a temperature range of 20-70 ° C. Added to the solid-liquid separation zone in
(D) mixing the water and optionally the extraction solvent, and the aqueous stream and the second aqueous stream in the mixing zone to form an aqueous mixture;
(E) adding an extraction solvent to the aqueous mixture in the extraction zone to form an extract stream and a raffinate stream; and (f) separating the extract stream in the separation zone to obtain a high boiling point organic impurity stream and a recovery extraction solvent Method of recovering a catalyst from a mother liquor comprising the steps of forming a stream . 前記工程（ａ）において、前記溶媒及び水の５０〜８０重量％を母液から除去する請求項２１に記載の方法。   22. The method of claim 21, wherein in step (a), 50-80% by weight of the solvent and water are removed from the mother liquor. 前記抽出ゾーンが向流抽出装置を含む請求項２１に記載の方法。   22. The method of claim 21, wherein the extraction zone comprises a countercurrent extraction device. 前記抽出ゾーンが一段抽出装置を含む請求項２1に記載の方法。   22. The method of claim 21, wherein the extraction zone comprises a single stage extractor. 前記溶媒高含有流が酢酸ｎ−プロピル、酢酸イソプロピル、酢酸イソブチル、酢酸ｓｅｃ−ブチル、酢酸エチル及び酢酸ｎ−ブチルからなる群から選ばれる溶媒を含む請求項２１に記載の方法。   22. The method of claim 21 wherein the solvent rich stream comprises a solvent selected from the group consisting of n-propyl acetate, isopropyl acetate, isobutyl acetate, sec-butyl acetate, ethyl acetate and n-butyl acetate.
JP2004168839A 2003-06-05 2004-06-07 Extraction method for removing impurity from carboxylic acid-synthesized mother liquor Pending JP2004358466A (en)

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US10/455,016 US7410632B2 (en) 2003-06-05 2003-06-05 Extraction process for removal of impurities from mother liquor in the synthesis of carboxylic acid

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EP (2) EP1484307A1 (en)
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KR (1) KR101169466B1 (en)
CN (1) CN1572765B (en)
AR (1) AR044616A1 (en)
BR (1) BRPI0401884A (en)
CA (1) CA2466999C (en)
ES (1) ES2437854T3 (en)
MX (1) MXPA04005328A (en)
MY (1) MY142041A (en)
PL (1) PL2292581T3 (en)
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